Phosphorus oxychloride → HCID 59312360, 화합물

HRID 2077053노트

반응식

HRID 2077053 반응식
P(Cl)(Cl)([Cl:3])=O.[CH2:6]([N:13]1[CH2:19][CH2:18][C:17]2[C:20](=O)[NH:21][C:22]([CH2:24][C:25]3[CH:30]=[CH:29][CH:28]=[C:27]([Cl:31])[CH:26]=3)=[N:23][C:16]=2[CH2:15][CH2:14]1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>[Cl-].C([N+](CC)(CC)CC)C.C(#N)CC>[CH2:6]([N:13]1[CH2:19][CH2:18][C:17]2[C:20]([Cl:3])=[N:21][C:22]([CH2:24][C:25]3[CH:30]=[CH:29][CH:28]=[C:27]([Cl:31])[CH:26]=3)=[N:23][C:16]=2[CH2:15][CH2:14]1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

참가 물질

5

반응물 2

HCID 24813Phosphorus oxychlorideHCID 136058092HCID 136058092, 화합물

생성물 1

HCID 59312360HCID 59312360, 화합물수율 87.7%

시약·촉매·용매 2

HCID 5946Tetraethylammonium Chloride촉매HCID 7854Propionitrile용매

반응 조건

온도
100 °C

실험 절차

Phosphoryl chloride (1.33 ml, 14.3 mmol) and tetra-ethyl ammonium chloride (472 mg, 2.85 mmol) were added to a solution of the product of Step A (361 mg, 0.95 mmol) in propionitrile (10 ml) and heated to 100° C. for 17 h. The reaction mixture was concentrated in vacuo then azeotroped with toluene then dichloromethane. The residue was partitioned between dichloromethane (30 ml) and water (20 ml), stirred for 30 min then the organic layer was separated, dried over magnesium sulphate and concentrated in vacuo to give the title compound as a foam in 87.7% yield, 332 mg.

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customthen azeotroped with toluene
  3. customThe residue was partitioned between dichloromethane (30 ml) and water (20 ml)
  4. customthe organic layer was separated
  5. dry with materialdried over magnesium sulphate
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-e199dbeaa8ed49efb3200f3aec78b74f
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07928099B2

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